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Process for syndiotactic polymerization of styrene

A polymerization method and technology of styrene, which is applied in the field of syndiotactic polymerization of styrene, can solve the problems of catalyst catalytic efficiency reduction, agglomeration, gel generation, etc.

Inactive Publication Date: 2006-10-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is that in the past, in the process of preparing syndiotactic polystyrene, agglomeration and gel are prone to occur, which reduces the catalytic efficiency of the catalyst, and a new method for syndiotactic polymerization of styrene is provided.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] On a 10-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 2375 grams of styrene monomer, at this time the temperature in the system is 40 ° C, inject 52.8 mmoles of triisobutylaluminum, 105.6 mmoles of MAO, 0.214 mmoles of Cp * Ti(OC 6 h 4 ) 3 The titanocene catalyst toluene solution, where Cp * It is pentamethylcyclopentadienyl. After the catalyst is added, gradually heat the jacket, and make the temperature in the system reach the polymerization temperature of 70°C in about 30 minutes. After stirring and reacting at 300 rpm for 4 hours, use ethanol-hydrochloric acid The solution stops the reaction, washes, and is dried to obtain 1950 grams of powder solids, substantially no lumps, catalyst efficiency of 154 kilograms of polymer / (gram of titanium), syndiotacticity of 97%, molecular weight distribution Mw / Mn=2.12, wherein Mw is the weight average Molecular weight, Mn is number average molecular weight.

Embodiment 2

[0015] On a 10-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 2375 grams of styrene monomer, at this time the temperature in the system is 45 ° C, inject 52.8 mmoles of triisobutylaluminum, 105.6 mmoles of MAO, 0.214 mmoles of Cp * Ti(OC 6 h 4 ) 3 Toluene solution of the titanocene catalyst, after the catalyst is added, gradually heat the jacket, make the temperature in the system reach the polymerization temperature of 70°C in about 40 minutes, stir and react at 300 rpm for 4 hours, then stop the reaction with ethanol-hydrochloric acid solution , washed and dried to obtain 1920 grams of powder solids, substantially no lumps, catalyst efficiency of 151 kilograms of polymer / (gram of titanium), syndiotacticity of 97%, molecular weight distribution Mw / Mn=2.15.

Embodiment 3

[0023] On a 10-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 2375 grams of styrene monomer, at this time, the temperature in the system is 35 ° C, inject 52.8 mmoles of triisobutylaluminum, 105.6 mmoles of MAO, 0.214 mmoles of Cp with a syringe * Ti(OC 6 h 4 -F) 3 Toluene solution of the titanocene catalyst, after adding the catalyst, gradually heat the jacket, make the temperature in the system reach the polymerization temperature of 75°C in about 40 minutes, stir and react at 300 rpm for 4 hours, then stop the reaction with ethanol-hydrochloric acid solution , washed and dried to obtain 1991 grams of powder solids, substantially no lumps, catalyst efficiency of 156 kilograms of polymer / (gram of titanium), syndiotacticity of 99%, molecular weight distribution Mw / Mn=2.16.

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Abstract

A process for the syndiotactic polymerization of styrene to prepare syndiotactic polystyrene features that the cyclopentadienyl titanium compound and alkylaluminium are used as catalyst, the catalyst is added at optimal reaction temp (5-40 deg.C) and the temp is raised to the optimal reaction temp within 10-60 min.

Description

technical field [0001] The present invention relates to a process for the syndiotactic polymerization of styrene. Background technique [0002] A homogeneous catalytic system composed of a titanocene compound and a cocatalyst methylaluminoxane (MAO) or a borofluorine compound is used for the syndiotactic polymerization of styrene to obtain a syndiotactic polymer with a syndiotactic degree of more than 96%. The melting point of the polymer is as high as 270°C, the crystallization speed is fast, the chemical resistance is good, the heat resistance is good, the molecular weight distribution is narrow, the dimensional stability is good, and it has excellent electrical properties. Its comprehensive properties can be compared with engineering plastics. The advent of syndiotactic polystyrene (SPS) has aroused people's research on its catalytic system, especially the metallocene compound as the main catalyst. Many highly active catalysts have come out...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F12/08C08F4/642
Inventor 沈志刚余波王荣伟赵薇薇张正国
Owner CHINA PETROLEUM & CHEM CORP